反应详情

温度

45 °C

At 45° C., a solution of 62.5 g [391 mmol] of bromine in 120 ml of glacial acetic acid is added dropwise over a period of 1 hour to a solution of 47.6 g [290 mmol] of 2,6-dimethylphenylacetic acid in 300 ml of glacial acetic acid. The reaction mixture is then stirred at 45° C. for another 16 hours and concentrated on a rotary evaporator. The solid obtained is stirred in 180 ml of methylcyclohexane at room temperature for 4 hours. After filtration, the residue is washed twice with in each case 60 ml of methylcyclohexane and then dried. This gives 64.9 g of a solid. GC(sil.) analysis: 97.7% pure (89.9% of theory).

1. concentrationconcentrated on a rotary evaporator
2. customThe solid obtained
3. filtrationAfter filtration
4. washthe residue is washed twice with in each case 60 ml of methylcyclohexane
5. customdried